반응 #5123

ord-603826e869b34924b60f03525d155479

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwhich was added to the above mixture over a period of 2 hours
  2. 2
    온도This reaction mixture was further heated at the boiling temperature for 2 hours
  3. 3
    온도cooled to the ambient temperature
  4. 4
    기타The residues obtained
  5. 5
    기타after removing the solvent from the mixture
  6. 6
    기타were purified by silica gel column chromatography

실험 절차

A mixture of 14.0 g of 3-methylbenzyl chloride and 50.0 g of ethyl acrylate dissolved in 300 ml of dry toluene was heated to 110° C. Separatively, 3.0 g of 2,2'-azobisisobutyronitrile(AIBN) and 32.0 g of tri-n-butyltin hydride were dissolved in 200 ml of dry toluene, which was added to the above mixture over a period of 2 hours. This reaction mixture was further heated at the boiling temperature for 2 hours and then cooled to the ambient temperature. The residues obtained after removing the solvent from the mixture were purified by silica gel column chromatography to provide ethyl-4-(3-methylphenyl)butanoate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05242944uspto-grants-1993_09